EP2995591B1 - Verfahren zur abwasserbehandlung - Google Patents

Verfahren zur abwasserbehandlung Download PDF

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Publication number
EP2995591B1
EP2995591B1 EP15183006.4A EP15183006A EP2995591B1 EP 2995591 B1 EP2995591 B1 EP 2995591B1 EP 15183006 A EP15183006 A EP 15183006A EP 2995591 B1 EP2995591 B1 EP 2995591B1
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EP
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Prior art keywords
wastewater
supernatant
concentration
organic compounds
steam
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EP15183006.4A
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English (en)
French (fr)
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EP2995591A1 (de
Inventor
Byung Joo Kim
Seong Tae Kim
Cholok Kim
Taekyun Yoo
Yang Ju Lee
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Hanwha Chemical Corp
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Hanwha Chemical Corp
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/02—Treatment of water, waste water, or sewage by heating
    • C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/02—Treatment of water, waste water, or sewage by heating
    • C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C02F1/048—Purification of waste water by evaporation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/02—Treatment of water, waste water, or sewage by heating
    • C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C02F1/16—Treatment of water, waste water, or sewage by heating by distillation or evaporation using waste heat from other processes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/32—Hydrocarbons, e.g. oil
    • C02F2101/322—Volatile compounds, e.g. benzene
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2301/00—General aspects of water treatment
    • C02F2301/06—Pressure conditions
    • C02F2301/063—Underpressure, vacuum

Definitions

  • the present invention relates to a method for treating wastewater which is discharged from an Aldol process consisting of the steps of performing an evaporative concentration of wastewater comprising non-biodegradable organic compounds and salt components at a concentration of 10,000 ppm or more to separate a supernatant to an upper part and a concentrate to a lower part; using a part of the supernatant as a steam for fuel, and degrading a remaining part of the supernatant by microorganisms, wherein a vacuum system is used for the evaporative concentration of the wastewater, wherein the wastewater has a pH greater than 6, wherein the method is without acid treatment or use of extractants. More specifically, the present invention relates to a method for treating wastewater capable of treating wastewater that comprises non-biodegradable organic compounds and a high concentration of salt components and thus is difficult to treat by microorganisms by an environmentally-friendly and low energy method.
  • wastewater comprising a high concentration of salt components, organic compounds or catalyst residue is generated as by-products.
  • an aldol condensation reaction which is industrially very important, refers to a process wherein linear or branched aldehyde is produced by reaction with olefin in the presence of a metal catalyst and ligand by hydroformylation known as an OXO-reaction, and then, alpha, beta-unsaturated aldehyde is produced through an aldol condensation reaction.
  • the produced alpha, beta-unsaturated aldehyde is used as starting material or intermediate for synthesis of many organic compounds. And, if the alpha, beta-unsaturated aldehyde is completely hydrogenated, monohydric saturated alcohol is produced.
  • the aldol condensation reaction is promoted by acid or base, and in the industrial process, base, particularly sodium hydroxide is used a lot.
  • the oxygen demand can be calculated by Chemical Oxygen Demand (COD).
  • COD Chemical Oxygen Demand
  • a microbial treatment plant as the contamination degree of wastewater is higher, oxygen demand increases, and for treating this, introduction of air in the wastewater should be increased, thus increasing energy consumption, or capacity expansion of treatment facilities is required. Otherwise, due to decrease in dissolved oxygen of the wastewater treatment facilities, death of microorganisms may be caused, or undesirable anaerobic degradation may be initiated.
  • EP 0631988 discloses a method of mixing wastewater from an aldol process with another washing water, and then, acidifying to pH 0 to 6, and separating the formed organic phase and extracting the aqueous phase together with 2-ethylhexanol. Wherein the treated wastewater is sent to a water purifying facilities, while separated and removed organic impurities are distilled to recover an extractant.
  • EP 0926100 suggested a process of adjusting various wastewater streams from the production of 2-ethylhexanal and 2-ethylhexanol to pH 0 to 6 separately or after being transferred, and then, separating and removing an organic phase. And then, the aqueous phase from which most organic impurities have been removed is extracted with 2-ethylhexanal, so as to separate and remove organic components still dissolved or dispersed therein.
  • this process also cannot avoid loss of 2-ethylhexanol.
  • EP 2 690 071 A1 provides a method for the treatment of alkaline wastewater comprising sodium ions and organic impurities, the method comprising the steps of a) contacting part of the wastewater with a cation exchange resin to obtain an acidic wastewater portion, b) mixing the acidic wastewater portion and the remaining wastewater portion optionally in the presence of a neutralizing solution to obtain an effluent having a pH of 5 to 9, and c) reducing the amount of the organic impurities from the effluent.
  • EP 2 508 489 A2 relates to a method of treating waste water produced during the nitration of compounds, which includes an appropriate pretreatment process and a vacuum evaporation process, so that acidic or alkaline aqueous waste water which is difficult to treat via conventional processes can be easily treated without performing microorganism treatment.
  • CN 102730894 A discloses a method for treating waste alkaline liquor produced in a butanol and octanol production device and belongs to the field of treatment on waste water produced by organic compound production.
  • the method is characterized by comprising the following steps of a, normal-pressure steam stripping, b, low-pressure evaporation concentration, c, acidification phase-separation, d, organic phase rectification, and e, simple evaporation concentration.
  • JP H01 262981 A discloses a method to perform waste water treatment efficiently, by adding alkali substances to waste water to effect reaction therebetween, guiding nonvolatile compounds and volatile compounds to be vaporized.
  • the present invention provides a method for treating wastewater which is discharged from an Aldol process consisting of the steps of performing an evaporative concentration of wastewater comprising non-biodegradable organic compounds and salt components at a concentration of 10,000 ppm or more to separate a supernatant to an upper part and a concentrate to a lower part; using a part of the supernatant as a steam for fuel, and degrading a remaining part of the supernatant by microorganisms, wherein a vacuum system is used for the evaporative concentration of the wastewater, wherein the wastewater has a pH greater than 6, wherein the method is without acid treatment or use of extractants.
  • wastewater comprising a high concentration of impurities such as salt components and non-biodegradable organic compounds generated in various organic chemical processes can be purified by low energy and simple process steps.
  • the treatment method of the present invention does not use a separate extractant for extracting impurities and does not require a pretreatment process such as acidification for oil/water separation and the like, and thus, the process is simple, and various problems due to the introduction of pH modifiers or extractants can be prevented.
  • the supernatant separated in the method for treating wastewater of the present invention can be used as steam for fuel of another process, total flux of discharged wastewater may be decreased, and simultaneously, energy may be further reduced, and treatment load of microbial degradation may be reduced, thus rendering the treatment method environmentally friendly.
  • each constructional element is formed “on” or “above” each construction element, it means that each constructional element is formed directly on each constructional element, or that other constructional elements may be additionally formed between the layers or on the object or substrate.
  • the method for treating wastewater which is discharged from an Aldol process of the present invention comprises the steps of performing an evaporative concentration of wastewater comprising non-biodegradable organic compounds and a high concentration of salt components to separate a supernatant to an upper part and a concentrate to a lower part; and using a part of the supernatant as a steam for fuel.
  • wastewater comprising non-biodegradable organic compounds and a high concentration of salt components is concentrated by evaporation.
  • wastewater means water that is discharged from an Aldol process and includes waste or impurities to be removed or degraded.
  • non-biodegradable organic compounds mean organic substances that are difficult to directly treat in a microbial wastewater treatment plant without an oil separation process such as acid treatment, extraction or evaporative concentration.
  • the salt components mean ions hindering microbial coagulation when wastewater is biologically treated, and representative examples thereof include monovalent cationic ions such as Na + or K + .
  • Wastewater to be treated in the present invention comprises such non-biodegradable organic compounds and thus has high COD, and comprises a high concentration of salt components such as a sodium salt (Na + ), and thus, is difficult to degrade by microorganisms even after acid treatment or treatment with an extractant.
  • salt components such as a sodium salt (Na + )
  • a microbial treatment system In case wastewater comprises non-degradable organic compounds at a high concentration, a microbial treatment system should be prepared on a large scale, requiring excessive operation cost of microbial treatment system, which is not preferable in terms of economic efficiency. And, if short of treatment capacity, growth and coagulation of microorganisms in the aeration tank of wastewater treatment system may be hindered, causing death of microorganisms due to decrease in dissolved oxygen.
  • the salt components are difficult to treat by microorganisms, and in case a high concentration of salt components are included in wastewater, they can be generally removed by the evaporative concentration; however, in this case, organic substances that have lower boiling point than water or form minimum azeotropic point lower than water are separated together the supernatant, thus requiring a separate oil/water separation process.
  • An industrial-scale chemical process inevitably discharges a significant amount of wastewater contaminated with organic/inorganic compounds such as by-products, organic solvents, catalyst residue, salts and the like.
  • the aldol process which is important in the industrial preparation process of alcohol, specifically includes an aldol addition reaction, an aldol condensation reaction of aldehyde and aldol, and an aldol condensation reaction of aldehyde and ketone.
  • an oxo reaction for preparing aldehyde which is raw material of aldol reaction
  • a catalyst preparation reaction for preparing a catalyst used for the oxo reaction, and the like waste water comprising a high concentration of non-biodegradable organic compounds and basic compounds such as sodium hydroxide (NaOH) is produced.
  • NaOH sodium hydroxide
  • Fig. 1 shows a flow chart of the wastewater treatment method of the conventional art.
  • Fig. 1 in the wastewater treatment method according to the conventional art, first, pretreatment of acidifying wastewater to separate into an organic phase and an aqueous phase is conducted.
  • the pretreated wastewater is sent to a wastewater treatment plant to treat by microorganisms (degradation of organic compounds), wastewater with decreased organic compounds is discharged, and solid waste made into the form of a cake by dehydration is sent to an additional treatment process.
  • microorganisms degradation of organic compounds
  • wastewater treatment system since even wastewater passing through pretreatment contains a high concentration of salt components and non-biodegradable organic compounds in large quantities, wastewater treatment system should be expanded to a large scale when treating by microorganisms, thus consuming high operation cost. And, in case wastewater comprising a large quantity of organic compounds is introduced in a wastewater treatment plant at a time, growth or coagulation of microorganisms in the aeration tank of the wastewater treatment plant may be hindered, and dissolved oxygen may decrease to cause death of microorganisms.
  • wastewater comprising non-biodegradable organic compounds and a high concentration of salt components is concentrated by evaporation before microbial degradation, and the supernatant with drastically decreased non-degradable organic compounds, from which salt components are substantially removed, is separated from the wastewater, thereby facilitating microbial degradation.
  • Fig. 2 shows a flow chart of the wastewater treatment method according to one example of the present invention.
  • an evaporative concentration process is conducted without introducing a pH modifier such as acid or base in wastewater.
  • the supernatant As the wastewater is firstly concentrated by evaporation, the supernatant is separated to an upper part of the column, and concentrate of organic compounds and salt components is separated to a lower part, and the supernatant becomes substantially free of salt components and non-biodegradable organic compounds.
  • a part of the supernatant stream may be separated, supplied to a heating furnace and used as a steam for fuel.
  • the supernatant as the steam for fuel, flux of wastewater to be treated is reduced, and furthermore, a small amount of organic compounds remaining in the supernatant is combusted to supply quantity of heat to other processes.
  • a part of the supernatant from which salt ingredients and non-biodegradable organic compounds are substantially removed is sent to a wastewater treatment plant, and discharged after conducting microbial degradation for the remaining organic compounds, and solid waste made in the form of a cake by dehydration is sent to an additional treatment process.
  • the supernatant introduced in the wastewater treatment plant includes drastically decreased organic compounds, microbial degradation is facilitated, thus reducing operation cost of wastewater treatment plant, and remarkably reducing the amount of generated solid waste.
  • the wastewater is wastewater generated in an aldol process or in a reaction for preparing raw material and/or catalyst used in the aldol process. Also disclosed is that it may be applied for all industrial wastewater that is generated from various chemical processes, and comprises non-biodegradable organic compounds and a high concentration of salt components and thus is difficult to directly degrade by microorganisms, or requires large treatment capacity.
  • the wastewater may comprise branched isomers of aldehyde, linear or branched alcohol having the same carbon number as aldehyde, linear or branched alcohol having one more carbon number than aldehyde.
  • the wastewater comprises sodium salt at a high concentration at about 10,000 ppm or more.
  • the wastewater is wastewater discharged from an aldol process, it has a basic pH greater than 6, for example greater than about 6 and about 14 or less.
  • the supernatant with decreased non-biodegradable organic compounds, from which salt components are substantially removed is separated to the upper part, and the concentrate of the non-biodegradable organic compounds and salt ingredients is separated to the lower part.
  • the apparatus for conducting the evaporative concentration is a vacuum system, and an evaporative concentrator commonly used in the technical field to which the invention pertains can be used.
  • the step of evaporative concentration of wastewater may be conducted by evaporating the wastewater in a column to which steam or waste heat discharged from another process is supplied as a heat source.
  • the temperature and the pressure of the supplied steam or waste heat are not specifically limited, and may be appropriately controlled so that the non-biodegradable organic compounds may be sufficiently decreased in the supernatant separated in the evaporative concentration process, and for example, steam of about 2.5 barg or less may be used as a heat source to conduct the evaporative concentration step.
  • the step of evaporative concentration of wastewater may be conducted by heating so that a temperature of steam of the supernatant may become about 80 °C or more, for example about 80 to 100°C.
  • consumption energy may be further reduced by lowering the pressure of a column to decrease the temperature and the amount of steam used as a heat source of the column, or by using waste heat discharged from another process as a heat source.
  • the evaporative concentration may be conducted under pressure condition of about -100 mmH 2 O to -10 mmH 2 O using vacuum system, and in this case, efficiency of evaporative concentration may further increase, and thus, required heat source may decrease and more wastewater may be treated.
  • the COD of the supernatant separated by the evaporative concentration may decrease to less than about 10%, or less than about 7%, or less than about 5% of the COD of wastewater before the evaporative concentration.
  • salt components may be substantially removed.
  • substantially removed means that in the supernatant, the salt components are not detectable or detected at a concentration of 10 ppm or less, or the salt components are removed about 99.9% to about 100%, or about 99.99% to about 100% compared to the concentration of the salt components included in the wastewater before the evaporative concentration.
  • the supernatant with remarkably decreased COD, from which salt components are substantially removed, may be easily treated by microorganisms.
  • a part of the supernatant from which salt components are substantially removed may be supplied to a heating furnace and used as steam for fuel, and the remaining part may be sent to a microbial treatment plant and further pass through a microbial degradation process.
  • the supernatant in case the supernatant is supplied to a heating furnace, it may be re-evaporated and pressurized using steam and the like, and supplied as an atomizing steam of a heating furnace using liquid fuel.
  • the supernatant as steam for fuel, flux of wastewater to be ultimately treated may be reduced, and furthermore, a small amount of organic compounds remaining in the supernatant may be combusted to supply quantity of heat to another process.
  • a partial stream of the supernatant was pressurized and 5.5barg steamed, and completely combusted and removed by using as atomizing steam in a reformer (furnace and the like), and the remaining stream was sent to a wastewater treatment plant, water passing through microbial degradation was finally discharged, and solid waste made in the form of a cake by dehydration was sent to an additional treatment process.
  • a reformer furnace and the like
  • a partial stream of the supernatant was pressurized and 5.5barg steamed, and completely combusted and removed by using as atomizing steam in a reformer (furnace and the like), and the remaining stream was sent to a wastewater treatment plant, water passing through microbial degradation was finally discharged, and solid waste made in the form of a cake by dehydration was sent to an additional treatment process.
  • a reformer furnace and the like
  • a sample and a standard solution were prepared as follows, and analyzed by AAS(Atomic Absorption-Spectrometry) at 589nm.
  • Example and Comparative Example for the wastewater, measurement was conducted after 5,000-fold dilution with distilled water, and for the supernatant after evaporative concentration, 50mL of the sample and 2.5 mL of a HCl solution were put, and the solution was made-up with distilled water so that the concentration of HCl became 2mol/L and then measurement was conducted.
  • a Na standard solution for AAS 1000mg/L of a Na standard solution for AAS was prepared into 0.5mg/L, 1.0mg/L solutions, each was taken, 10mL of a HCl solution was added thereto, and the solution was made-up with distilled water so that the concentration of HCl became 2mol/L.
  • COD mg / mL b ⁇ a ⁇ f ⁇ 1000 / V ⁇ 0.2
  • the COD (Cr) of the sample was measured according to ASTM D1252 (11.02) by a standard test method.
  • Example 1 Wastewater 13.2 12,840 10,240 121,300 Supernatant after evaporative concentration 3.6 ⁇ 0.2 627 3140
  • Example 2 Wastewater 5.9 18,980 12,890 65,800 Supernatant after evaporative concentration 3 ⁇ 0.1 774 4920 *not claimed

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  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Organic Chemistry (AREA)
  • Heat Treatment Of Water, Waste Water Or Sewage (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Biodiversity & Conservation Biology (AREA)
  • Microbiology (AREA)

Claims (4)

  1. Verfahren zur Behandlung von aus einem Aldol-Prozess abgeführten Abwasser, bestehend aus den Schritten des
    Durchführens einer Eindampfung von Abwasser, das nicht biologisch abbaubare organische Komponenten und Salzkomponenten mit einer Konzentration von 10.000 ppm oder mehr umfasst, zur Trennung eines Überstands in einen oberen Teil und eines Konzentrats in einen unteren Teil;
    Verwendens eines Teils von dem Überstand als Dampf für Heizstoff und
    Abbauens eines verbleibenden Teils des Überstands durch Mikroorganismen,
    wobei ein Vakuumsystem zur Eindampfung des Abwassers verwendet wird, wobei das Abwasser einen pH-Wert von mehr als 6 aufweist, wobei das Verfahren ohne Säurebehandlung oder Verwendung von Extraktionsmitteln erfolgt.
  2. Verfahren zur Behandlung von Abwasser nach Anspruch 1, wobei der Überstand nach dem erneuten Verdampfen und Druckbeaufschlagen als Zerstäuberdampf eingesetzt wird.
  3. Verfahren zur Behandlung von Abwasser nach Anspruch 1, wobei die Salzkomponente Natriumsalz (Na+) enthält.
  4. Verfahren zur Behandlung von Abwasser nach Anspruch 1, wobei das Abwasser unter Verwendung von Dampf oder Abwärme eingedampft wird.
EP15183006.4A 2014-08-28 2015-08-28 Verfahren zur abwasserbehandlung Active EP2995591B1 (de)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109650345B (zh) * 2018-04-09 2022-03-04 西南科技大学 一种石膏中硫钙资源分别利用的方法
CN109741849B (zh) * 2018-12-27 2023-06-16 中核四0四有限公司 一种铀纯化转化含铀含氟废液的深度净化方法
WO2021037572A1 (en) 2019-08-23 2021-03-04 Basf Se Process for treating wastewater from an aldolization process
JP7303493B2 (ja) * 2019-10-21 2023-07-05 住友金属鉱山株式会社 Ｃｏｄ測定装置
CN113562918B (zh) * 2021-08-09 2023-04-18 天俱时工程科技集团有限公司 含锰的高浓度有机废水的处理方法

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JPH01262981A (ja) * 1988-04-12 1989-10-19 Nittetsu Kakoki Kk 有機酸性物質を含む廃水の処理方法
EP2508489A2 (de) * 2009-12-01 2012-10-10 Huchems Fine Chemical Corp. Verfahren zur behandlung von während der herstellung von nitroverbindungen produziertem abwasser
CN102730894A (zh) * 2011-04-15 2012-10-17 中国石油化工股份有限公司 丁辛醇生产装置中产生的废碱液的处理方法

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EP2508489A2 (de) * 2009-12-01 2012-10-10 Huchems Fine Chemical Corp. Verfahren zur behandlung von während der herstellung von nitroverbindungen produziertem abwasser
CN102730894A (zh) * 2011-04-15 2012-10-17 中国石油化工股份有限公司 丁辛醇生产装置中产生的废碱液的处理方法

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